CN113547131B - Silver powder with rough surface and multi-mesoporous structure inside and preparation method thereof - Google Patents
Silver powder with rough surface and multi-mesoporous structure inside and preparation method thereof Download PDFInfo
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- CN113547131B CN113547131B CN202110802401.9A CN202110802401A CN113547131B CN 113547131 B CN113547131 B CN 113547131B CN 202110802401 A CN202110802401 A CN 202110802401A CN 113547131 B CN113547131 B CN 113547131B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
Abstract
The invention discloses a preparation method of multi-mesoporous silver powder, which comprises the following steps: step 1: preparing silver nitrate solution, adding a dispersing agent, and uniformly stirring to form silver nitrate dispersion liquid; step 2: adding a reducing agent and a silanization reagent into the silver nitrate dispersion liquid; step 3: suction filtering and washing are carried out on the silver slurry to obtain wet silver powder; step 4: adding wet silver powder into alkaline solution, filtering and washing; step 5: coating the silver powder surface subjected to alkali treatment in the step 4 with a coating agent, wherein the coating agent contains paraformaldehyde, drying after coating, crushing by using an airflow crusher, and sieving by ultrasonic vibration to obtain the multi-mesoporous silver powder. According to the invention, the silanization reagent is creatively introduced as a mesoporous template agent, and paraformaldehyde is introduced into the dispersing agent with silver powder as a surface coating, so that the silver powder with a rough surface and a multi-mesoporous structure inside is prepared by slowly decomposing the silver powder at normal temperature, the prepared silver powder has high surface activity, and the electrical property of the silver paste on the front side of solar energy is improved.
Description
Technical Field
The invention relates to the technical field of new energy materials, in particular to silver powder with rough surface and multi-mesoporous structure inside and a preparation method thereof.
Background
Along with the industrialization development of the photovoltaic for nearly 20 years, the photovoltaic becomes one of the best choices of new energy power generation, and also gradually becomes a strategic emerging industry with great advantages in China. According to the recently issued new energy planning of the country: the fourteen five renewable energy source planning up-regulates the proportion of non-fossil energy sources, exceeds market expectations and is estimated to reach 20% in 2030. Meanwhile, under the guidance of 'carbon neutralization', 55-65GW is expected to be newly installed in 2021 domestic, and 70-90GW is expected to be newly installed in annual average photovoltaic in China in a 'fourteen-five' period. Under the background, the solar cell has the advantages of cost reduction, synergy and reduction of the application cost. Silver paste is used as a noble metal paste for printing on solar cell silicon wafers. The main composition of the silver paste is glass powder, silver powder and an organic carrier, wherein the silver powder accounts for more than 85 percent. Therefore, the silver powder performance determines the quality of silver paste to a certain extent, and solar positive silver powder suppliers with better performance on the market mainly comprise the same company in japan, AMES in the united states, schmest in China, jingxin, jianbang and the like. From the patents and the existing documents of the manufacturers, the redox method can be seen, and the reducing agent is basically as follows: formaldehyde, glucose, hydroquinone, hydrazine hydrate, phosphorous acid, ascorbate, and the like; meanwhile, the prepared silver powder has smoother surface and lower activity, and the prepared silver has wider line type, too low aspect ratio and large shading area after being sintered at high temperature, so that the current is lower; (2) meanwhile, in the silver powder preparation process, more dispersing agents are used for coating the silver powder, so that aggregation among the silver powder is reduced; the surface of the silver powder obtained after drying contains 0.2 to 0.6 mass percent of dispersing agent, and the dispersing agent is generally difficult to decompose, so that the mutual contact surface between the silver powder is hindered, and a certain line resistance is increased; meanwhile, the glass powder is prevented from being directly contacted with silver powder to a certain extent, and the corresponding Rs value of the contact resistance is influenced.
Therefore, development of silver powder with high surface activity and better aspect ratio in the sintering process and easy decomposition of the surface coating agent at a lower temperature is urgently required, and reliable guarantee is provided for further improving the electrical performance of the solar front silver paste.
Disclosure of Invention
Based on the technical problems, the invention provides a preparation method of silver powder with rough surface and multi-mesoporous structure inside, which comprises the following steps:
step 1: preparing a silver nitrate solution, adding a dispersing agent into the silver nitrate solution, and uniformly stirring to form a silver nitrate dispersion liquid;
step 2: adding a reducing agent and a silanization reagent into the silver nitrate dispersion liquid to enable the silver nitrate and the reducing agent to undergo a reduction reaction to form silver slurry;
step 3: carrying out suction filtration on the silver slurry, and washing a solid phase with deionized water to obtain wet silver powder;
step 4: adding wet silver powder into an alkaline solution, removing silicon components in the silver powder, filtering, and washing a solid phase with deionized water until a washed liquid is neutral;
step 5: coating the silver powder surface subjected to alkali treatment in the step 4 with a coating agent, wherein the coating agent contains paraformaldehyde, drying, crushing by using an airflow crusher, and sieving by ultrasonic vibration to obtain the multi-mesoporous silver powder.
Further, in the silver nitrate solution, the concentration of silver nitrate is 2-4 mol/L, and the balance is water.
Further, the dispersing agent is one of stearic acid, oleic acid and polypropylene glycol, and the adding amount of the dispersing agent and the proportion of the silver nitrate solution are 6-10 g of the dispersing agent/1L of the silver nitrate solution.
Further, the silylation reagent is any one of a chlorosilane reagent and an alkoxy silane reagent; the addition amount of the reducing agent and the silylating agent and the proportion of the silver nitrate solution are 100-300 g of the reducing agent: 20-60 g of silylating agent: 1L of silver nitrate solution.
Further, the alkaline solution is ammonia water or sodium hydroxide solution, and the solubility of the solute in the alkaline solution is 0.1-0.2 mol/L.
Further, the coating agent is isopropanol solution of stearic acid, the mass percentage content of the stearic acid is 8% -10%, and the concentration of paraformaldehyde in the coating agent is 0.1-0.2 mol/L.
From the above technical scheme, the invention has the advantages that: the invention creatively introduces the mesoporous template agent as the structure guiding agent to prepare the silver powder with rough surface and multi-mesoporous structure inside, the prepared silver powder has high surface activity and can be well contacted at a lower temperature, and meanwhile, the surface coating agent is easy to decompose at the lower temperature, so that the electrical property of the silver paste on the front side of the solar energy is further improved.
Drawings
Fig. 1 is an SEM electron micrograph of silver powder prepared by the method described in example 1 and comparative example 2.
Detailed Description
The following is a detailed description of embodiments:
example 1
A preparation method of multi-mesoporous silver powder comprises the following steps:
step 1: preparing 5L of 3mol/L silver nitrate solution, adding 30g of stearic acid into the solution, and uniformly stirring to form silver nitrate dispersion liquid;
step 2: slowly adding 500g of reducing agent and 100g of silanization reagent solution into the silver nitrate dispersion liquid to enable the silver nitrate and the reducing agent to undergo a reduction reaction to form silver slurry, and simultaneously enabling the silanization reagent to serve as a nucleating agent to enable silver to be deposited on the silanization reagent; wherein the silylating agent is a chlorosilane agent;
step 3: filtering the silver slurry, and repeatedly washing and filtering the silver slurry with deionized water for 5 times to obtain wet silver powder;
step 4: soaking the obtained wet silver powder in 0.5mol/L sodium hydroxide aqueous solution for 1h, removing silicon components in the silver powder, and continuously washing until the pH value is neutral;
step 5: coating the surface of the silver powder subjected to alkali treatment in the step 4 by using a coating agent, wherein the coating agent contains paraformaldehyde, the coating agent is isopropanol solution of stearic acid, the mass percent of stearic acid is 10%, the concentration of the paraformaldehyde in the coating agent is 0.1mol/L, drying after coating, crushing by using an airflow crusher, and sieving by ultrasonic vibration to obtain the silver powder. SEM electron micrographs of the silver powder prepared in this example are shown in fig. 1.
Example 2
A preparation method of multi-mesoporous silver powder comprises the following steps:
step 1: preparing 5L of 3mol/L silver nitrate solution, adding 40g of oleic acid into the solution, and uniformly stirring to form silver nitrate dispersion liquid;
step 2: slowly adding 500g of reducing agent and 200g of silylating agent solution into the silver nitrate dispersion liquid to enable the silver nitrate and the reducing agent to undergo a reduction reaction to form silver slurry, and simultaneously enabling the silylating agent to serve as a nucleating agent to enable silver to be deposited on the silylating agent; wherein the silylating agent is a chlorosilane agent;
step 3: filtering the silver slurry, and repeatedly washing and filtering the silver slurry with deionized water for 5 times to obtain wet silver powder;
step 4: soaking the obtained wet silver powder in 0.5mol/L sodium hydroxide aqueous solution for 1h, removing silicon components in the silver powder, and continuously washing until the pH value is neutral;
step 5: coating the surface of the silver powder subjected to alkali treatment in the step 4 by using a coating agent, wherein the coating agent contains paraformaldehyde, the coating agent is isopropanol solution of stearic acid, the mass percent of stearic acid is 10%, the concentration of the paraformaldehyde in the coating agent is 0.1mol/L, drying after coating, crushing by using an airflow crusher, and sieving by ultrasonic vibration to obtain the silver powder.
Example 3
A preparation method of multi-mesoporous silver powder comprises the following steps:
step 1: preparing 5L of 3mol/L silver nitrate solution, adding 50g of dispersant polypropylene glycol into the solution, and uniformly stirring to form silver nitrate dispersion;
step 2: slowly adding 500g of reducing agent and 300g of silylating agent solution into the silver nitrate dispersion liquid to enable the silver nitrate and the reducing agent to undergo a reduction reaction to form silver slurry, and simultaneously enabling the silylating agent to serve as a nucleating agent to enable silver to be deposited on the silylating agent; wherein the silylating agent is an alkoxysilane agent;
step 3: filtering the silver slurry, and repeatedly washing and filtering the silver slurry with deionized water for 5 times to obtain wet silver powder;
step 4: soaking the wet silver powder in 0.5mol/L sodium hydroxide aqueous solution for 1h, removing silicon components in the silver powder, and continuously washing until the pH value is neutral;
step 5: coating the surface of the silver powder subjected to alkali treatment in the step 4 by using a coating agent, wherein the coating agent contains paraformaldehyde, the coating agent is isopropanol solution of stearic acid, the mass percent of stearic acid is 10%, the concentration of the paraformaldehyde in the coating agent is 0.1mol/L, drying after coating, crushing by using an airflow crusher, and sieving by ultrasonic vibration to obtain the silver powder.
Comparative example 1
A preparation method of silver powder comprises the following steps:
step 1: preparing 5L of 3mol/L silver nitrate solution, adding 30g of stearic acid into the solution, and uniformly stirring to form silver nitrate dispersion liquid;
step 2: slowly adding 500g of conventional reducing agent into the silver nitrate dispersion liquid to enable the silver nitrate and the reducing agent to undergo a reduction reaction to form silver slurry, wherein the conventional reducing agent is ascorbic acid;
step 3: filtering the silver slurry, and repeatedly washing and filtering the silver slurry with deionized water for 5 times to obtain wet silver powder;
step 4: coating the wet silver powder obtained in the step 3 by using a dispersing agent, wherein the coating agent contains paraformaldehyde, the coating agent is isopropanol solution of stearic acid, the mass percentage content of the stearic acid is 10%, the concentration of the paraformaldehyde in the coating agent is 0.1mol/L, drying after coating, crushing by using a jet mill, and sieving by ultrasonic vibration to obtain the silver powder.
Comparative example 2
A preparation method of silver powder comprises the following steps:
step 1: preparing 5L of 3mol/L silver nitrate solution, adding 30g of stearic acid into the solution, and uniformly stirring to form silver nitrate dispersion liquid;
step 2: slowly adding 500g of reducing agent into the silver nitrate dispersion liquid to enable the silver nitrate and the reducing agent to undergo a reduction reaction to form silver slurry; wherein the reducing agent is formaldehyde;
step 3: filtering the silver slurry, and repeatedly washing and filtering the silver slurry with deionized water for 5 times to obtain wet silver powder;
step 4: coating the wet silver powder obtained in the step 3 by using a dispersing agent, wherein the coating agent contains paraformaldehyde, the coating agent is isopropanol solution of stearic acid, the mass percentage content of the stearic acid is 10%, the concentration of the paraformaldehyde in the coating agent is 0.1mol/L, drying after coating, crushing by using a jet mill, and sieving by ultrasonic vibration to obtain the silver powder. SEM electron micrographs of the silver powder prepared in this comparative example are shown in fig. 1.
Comparative example 3
A preparation method of silver powder comprises the following steps:
step 1: preparing 5L of 3mol/L silver nitrate solution, adding 30g of stearic acid into the solution, and uniformly stirring to form silver nitrate dispersion liquid;
step 2: slowly adding 500g of conventional reducing agent and 100g of silanization reagent solution into the silver nitrate dispersion liquid to enable the silver nitrate and the reducing agent to undergo a reduction reaction to form silver slurry, and simultaneously enabling the silanization reagent to serve as a nucleating agent to enable silver to be deposited on the silanization reagent; wherein the silylating agent is a chlorosilane agent;
step 3: filtering the silver slurry, and repeatedly washing and filtering the silver slurry with deionized water for 5 times to obtain wet silver powder;
step 4: soaking the wet silver powder in 0.5mol/L sodium hydroxide aqueous solution for 1h, removing silicon components in the silver powder, and continuously washing until the pH value is neutral;
step 5: coating the surface of the silver powder subjected to alkali treatment in the step 4 by using a coating agent, wherein the coating agent contains paraformaldehyde, the coating agent is isopropanol solution of stearic acid, the mass percent of stearic acid is 10%, the concentration of the paraformaldehyde in the coating agent is 0.1mol/L, drying after coating, crushing by using an airflow crusher, and sieving by ultrasonic vibration to obtain the silver powder.
Example 4
The silver powders prepared in example 1 and comparative examples 1 to 3 were respectively tested to prepare front-side silver pastes, which were screen-printed onto silicon wafers, and the electrical properties thereof were tested, and the results are shown in the following table. Wherein experimental group comparative example 1 represents the electrical properties after silver paste made of silver powder prepared by the method described in comparative example 1 is printed on a silicon wafer, experimental group comparative example 2 represents the electrical properties … … after silver paste made of silver powder prepared by the method described in comparative example 2 is printed on a silicon wafer, and so on.
As is well known in the technical field, the technical difficulty of improving the efficiency by 0.05% is high, and the method successfully introduces a mesoporous structure into silver powder by introducing a silanization reagent as a mesoporous template agent and then removing the template agent by alkali, so that the silver powder with a rough surface and a multi-mesoporous structure inside is prepared, the silver paste with the multi-mesoporous silver powder, which is prepared into front silver paste, is screen-printed on a silicon wafer, and a silver grid line has large linear shrinkage in the sintering process, has a good aspect ratio and small shading area, so that the improvement of current Isc is high and the efficiency is high; on the other hand, paraformaldehyde can be coated on the surface of silver powder in the silver powder coating process, so that the surface of the silver powder becomes rough due to slow decomposition, and good ohmic contact is formed with a silicon wafer more easily in the silver grid line sintering process, so that the contact resistance is reduced, and the efficiency is improved.
The foregoing detailed description of the embodiments of the present invention will be provided to those skilled in the art, and the detailed description and the examples should not be construed as limiting the invention.
Claims (5)
1. The preparation method of the silver powder with the rough surface and the multi-mesoporous structure inside is characterized by comprising the following steps:
step 1: preparing a silver nitrate solution, adding a dispersing agent into the silver nitrate solution, and uniformly stirring to form a silver nitrate dispersion liquid;
step 2: adding a reducing agent and a silanization reagent into the silver nitrate dispersion liquid to enable the silver nitrate and the reducing agent to undergo a reduction reaction to form silver slurry; wherein the silylating agent acts as a mesoporous templating agent and a nucleating agent; the silanization reagent is any one of a chlorosilane reagent and an alkoxy silane reagent; the addition amount of the reducing agent and the silylating agent and the proportion of the silver nitrate solution are 100-300 g of the reducing agent: 20-60 g of silylating agent: 1L of silver nitrate solution;
step 3: carrying out suction filtration on the silver slurry, and washing a solid phase with deionized water to obtain wet silver powder;
step 4: adding wet silver powder into an alkaline solution, removing silicon components in the silver powder, filtering, and washing a solid phase with deionized water until a washed liquid is neutral;
step 5: coating the silver powder surface subjected to alkali treatment in the step 4 with a coating agent, wherein the coating agent contains paraformaldehyde, drying, crushing by using an airflow crusher, and sieving by ultrasonic vibration to obtain the multi-mesoporous silver powder.
2. The method for preparing silver powder with a rough surface and a multi-mesoporous structure in the silver powder according to claim 1, wherein the concentration of silver nitrate in the silver nitrate solution is 2-4 mol/L, and the balance is water.
3. The method for preparing silver powder with a rough surface and a multi-mesoporous structure in the silver powder according to claim 1, wherein the dispersing agent is one of stearic acid, oleic acid and polypropylene glycol, and the ratio of the adding amount of the dispersing agent to the silver nitrate solution is 6-10 g of the dispersing agent/1L of the silver nitrate solution.
4. The method for preparing silver powder with a rough surface and a multi-mesoporous structure in the silver powder according to claim 1, wherein the alkaline solution is ammonia water or sodium hydroxide solution, and the solubility of solute in the alkaline solution is 0.1-0.2 mol/L.
5. The method for preparing silver powder with a rough surface and a multi-mesoporous structure in the silver powder according to claim 1, wherein the coating agent is isopropanol solution of stearic acid, the mass percentage of the stearic acid is 8% -10%, and the concentration of paraformaldehyde in the coating agent is 0.1-0.2 mol/L.
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WO2012063747A1 (en) * | 2010-11-08 | 2012-05-18 | ナミックス株式会社 | Metal particles and manufacturing method for same |
CN103039521B (en) * | 2011-10-11 | 2014-11-05 | 国家纳米科学中心 | Method for preparing antibacterial powder loaded with monodisperse silver nanometer mesoporous silica |
JP5895552B2 (en) * | 2012-01-23 | 2016-03-30 | 住友金属鉱山株式会社 | Silver powder and method for producing the same |
CN103149194B (en) * | 2013-02-28 | 2015-08-26 | 西安交通大学 | A kind of preparation method of Surface enhanced raman spectroscopy matrix |
CN106448808A (en) * | 2016-12-12 | 2017-02-22 | 北京市合众创能光电技术有限公司 | Knotless screen printing front side silver paste for crystalline silicon solar cells |
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